An analytical scheme for determining various forms of sulphur in oil shales and associated rocks is presented. Acid-soluble sulphate, sulphur contained in monosulphide and in disulphide minerals, and organically-bound sulphur are all quantitatively recovered as separate fractions. Finely-ground oil-shale samples are treated in an inert atmosphere with 6M hydrochloric acid to dissolve the acid-soluble sulphate minerals and form H2S from the decomposition of monosulphide minerals. The acid-soluble sulphate is precipitated as barium sulphate and the H2S is collected and weighed as silver sulphide. Disulphide minerals in the solid residue from the acid treatment are reduced by an acidified Cr(II) solution in an inert atmosphere, releasing the sulphide as H2S. The H2S is collected as silver sulphide. An Eschka fusion oxidizes and solubilizes all sulphur remaining within the Cr(II)-treated residue. This sulphate represents organically-bound sulphur and is collected as barium sulphate. The analytical procedures have been verified by using 57Fe Mo??ssbauer spectroscopy. Good agreement between the chemical and Mo??ssbauer data substantiated the sequential removal of the forms of sulphur and also demonstrated the ability of Mo??ssbauer spectroscopy to determine the absolute quantities of iron present in specific minerals. ?? 1986.